Polychloral and process of making same.



TJNKTED STATES Patented Leugust 30, 1904.

PATENT EEicE.

POLYCHLORAL AND PROCESS OF MAKING SAME.

SPECIFICATION forming part of Letters Patent No. 768,744, dated August30, 1904.

Application filed May 6, 1904. Serial No. 206,774. (No specimens.)

To all whom, it may concern.-

Be it known that I, SIMON GliRTNER, chemist, a subject of the GermanEmperor, residing at Halle-on-the-Saale, Germany, (and whose post-officeaddress is 40 Albrechtstrasse, Halleon-the-Saale, Germany,) haveinvented acertain new and useful Process for the Manufacture ofPolychloral, (for which I have applied for a patent in Germany on the7th day of August, 1903,) of which the following is a specification.

According to the Ava Milan (Zc r Chem/dc (171, 7 6) Meyer and Dulk havecaused liquid trimethyl-amin to act on chloral, and thereby produced asolid mass which they assumed to consist of a mixture of severalpolymeric chlorals. The production of the reaction contained anadmixture of an adhesive substance which could not be removed withoutcausing decomposition of the entire product. Consequently it was notpracticable to obtain the original product of the reaction betweenchloral and trimethyl-amin in a pure state.

I have discovered that a homogeneous and stable polychloral, (CBOHCIQX,may be obtained by causing trimethyl-amin or other amins to act onchloral in the cold and treating the product with acids, whichpolychloral has hypnotic properties and is a very useful soporific. Thedetails of procedure for the manufacture of polychloral may, forinstance, be as follows: Ghloral is treated with pyridin by adding thelatter in drops while stirring and energetically cooling with ice untilthe mass begins to solidify, after which the stirring is continued untilthe mass has become quite hard. Subsequently the snow-white mass israpidly broken up into small particles and shaken with about half itsweight of dilute hydrochloric or other acid for about fifty minutes. Theliquid is separated from the insoluble residue by suction and the latterwashed with cold water until the washing-water no longer becomes acid.

The product thus obtained is subjected to pressure to remove anyremnants of liquid, after which it is broken up into small particles anddried, preferably in cacao, over concentrated sulfuric acid orphosphorus pentoxid. Instead of pyridin other aminsfor instance,allyl-aminsmay be used for polymerizing the chloral. The polymerizationof chloral may also be effected in the presence of chemically-inertsolvents. Chloral may, for instance, be dissolved in an equal weight ofpetroleum spirit, ether, or chloroform, after which a solution ofdimethyl-amin (two per cent. of the weight of chloral) in the samesolvent is added while cooling, and the mixture is allowed to stand inthe cold for abouttwo hours, during which time a solid white substanceseparates out, which is then drained. The purification of the product isagain efliected by shaking it with acids. Instead of dimethylamintrimethyl-amin may be used for polymerizing the chloral.

The polychloral obtained by the process described is a white solidsubstance which has a faint odor of chloral and differs from thepolymeric chlorals already known by the fact of its being slowly solublein water and alcohol already at ordinary temperature and more rapidly onheating, chloralhydrate or chloralalcoholate being formed at the sametime. When heated, it evaporates without melting. and it volatilizesslowly already at ordinary temperature. By alkalies it is split up intochloroform andformic acid. It has marked hypnotic properties and actsalso as an anesthetic, and it is less poisonous than chloralhydrate.

What I claim is 1. The process for the manufacture of a polychloral,which consists in causing chloral to act on an amin, While cooling. andtreating the solid product thus obtained with dilute acid, substantiallyas described.

2. The process for the manufacture of a polychloral, which consists inadding to chloral pyridin in drops, while cooling and stirring, untilthe mass begins to solidify, again stirring until the mass has becomequite solid, then breaking up the mass into particles, thoroughlyshaking it with dilute hydrochloric acid, separating the liquid. fromthe soluble residue, washing the latter and drying, substantially asdescribed.

3. As a new article of manufacture, a polychloral, consisting of a solidand slightly volatile hypnotic and anesthetic substance, slowly InWitness whereof I have signed this specisoluble in cold Water and incold alcohol, more fication in the presence of two subscribing wit- IOrapidly soluble in hot Water and. hot alcohol, nesses.,

while forming chloralhydrate or chloral alcol r1 7 5 holate, capable ofevaporation by heat with SIMON (TARlNEh out melting, and capable ofbeing split up by In presence of* alkalies into chloroform and formicacid, sub- KARL MAN'rsoH, stantially as described. GUSTAV NIGOLAI.

